Metal traces, analysis Fluorescence

Inorganic extractables/leachables would include metals and other trace elements such as silica, sodium, potassium, aluminum, calcium, and zinc associated with glass packaging systems. Analytical techniques for the trace analysis of these elements are well established and include inductively coupled plasma—atomic emission spectroscopy (ICP-AES), ICP-MS, graphite furnace atomic absorption spectroscopy (GFAAS), electron microprobe, and X-ray fluorescence. Applications of these techniques have been reviewed by Jenke. " An example of an extractables study for certain glass containers is presented by Borchert et al. ". ... 

X-ray fluorescence spectrometry, gas chromatography and neutron activation analysis (NAA). An older book edited by Hofstader, Milner and Runnels on Analysis of Petroleum for Trace Metals (1976), includes one chapter each on principles of trace analysis and techniques of trace analysis and others devoted to specific elements in petroleum products. Markert (1996) presents a fresh approach to sampling, sample preparation, instrumental analysis, data handling and interpretation. The Handbook on Metals in Clinical and Analytical Chemistry, edited by Seiler,... 

Knoechel, A., Prange, A., 1980. Analysis of trace elements in seawater. Part II. Determinaton of heavy metal traces in sea water by X-ray fluorescence analysis with totally reflecting sample holders. Microchim. Acta (Wien) II, 395 08. 

Hg from melted ice was measured by reduction to Hg(0), which was purged from solution by bubbling Ar gas. Hg(g) was trapped by metallic Au coated on sand. (Mercury is soluble in gold.) For analysis, the trap was heated to liberate Hg, which passed into a cuvet. The cuvet was irradiated with a mercury lamp, and fluorescence from Hg vapor was observed. The detection limit was 0.04 ng. Blanks prepared by performing all steps with pure water in place of melted glacier had 0.66 0.25 ng Hg/L, which was subtracted from glacier readings. All steps in trace analysis are carried out in a scrupulously clean environment. 

Chemical Properties. Elemental analysis, impurity content, and stoichiometry are determined by chemical or iastmmental analysis. The use of iastmmental analytical methods (qv) is increasing because these ate usually faster, can be automated, and can be used to determine very small concentrations of elements (see Trace AND RESIDUE ANALYSIS). Atomic absorption spectroscopy and x-ray fluorescence methods are the most useful iastmmental techniques ia determining chemical compositions of inorganic pigments. Chemical analysis of principal components is carried out to determine pigment stoichiometry. Analysis of trace elements is important. The presence of undesirable elements, such as heavy metals, even in small amounts, can make the pigment unusable for environmental reasons. 

Zinc smelters use x-ray fluorescence spectrometry to analyze for zinc and many other metals in concentrates, calcines, residues, and trace elements precipitated from solution, such as arsenic, antimony, selenium, tellurium, and tin. X-ray analysis is also used for quaUtative and semiquantitative analysis. Electrolytic smelters rely heavily on AAS and polarography for solutions, residues, and environmental samples. 

The detection and determination of traces of cobalt is of concern in such diverse areas as soflds, plants, fertilizers (qv), stainless and other steels for nuclear energy equipment (see Steel), high purity fissile materials (U, Th), refractory metals (Ta, Nb, Mo, and W), and semiconductors (qv). Useful techniques are spectrophotometry, polarography, emission spectrography, flame photometry, x-ray fluorescence, activation analysis, tracers, and mass spectrography, chromatography, and ion exchange (19) (see Analytical TffiTHODS Spectroscopy, optical Trace and residue analysis). 

Bromo-2-pyridyla2o)-5-diethylamiQophenol (5-Br-PADAP) is a very sensitive reagent for certain metals and methods for cobalt have been developed (23). Nitroso-naphthol is an effective precipitant for cobalt(III) and is used in its gravimetric determination (24,25). Atomic absorption spectroscopy (26,27), x-ray fluorescence, polarography, and atomic emission spectroscopy are specific and sensitive methods for trace level cobalt analysis (see... 

Wetai Ion Analysis. We have reported a sensitive trace-metal analysis based upon HPLC separation of p-aminophenyl EDTA chelates and fluorescence detection by postcolumn reaction with fluorescamine (23). An application of the pyridone chemistry already discussed leads to a fluorescent-labeled EDTA (VIII). 

Chong et al. [742] have described a multielement analysis of multicomponent metallic electrode deposits, based on scanning electron microscopy with energy dispersive X-ray fluorescence detection, followed by dissolution and ICP-MS detection. Application of the method is described for determination of trace elements in seawater, including the above elements. These elements are simultaneously electrodeposited onto a niobium-wire working electrode at -1.40 V relative to an Ag/AgCl reference electrode, and subjected to energy dispersive X-ray fluorescence spectroscopy analysis. Internal standardisation... 

Contrast the type of information obtainable in the determination of trace metals by X-ray fluorescence and electron probe analysis. 

Vukjovic et al.199 recently proposed a simple, fast, sensitive, and low-cost procedure based on solid phase spectrophotometric (SPS) and multicomponent analysis by multiple linear regression (MA) to determine traces of heavy metals in pharmaceuticals. Other spectroscopic techniques employed for high-throughput pharmaceutical analysis include laser-induced breakdown spectroscopy (LIBS),200 201 fluorescence spectroscopy,202 204 diffusive reflectance spectroscopy,205 laser-based nephelometry,206 automated polarized light microscopy,207 and laser diffraction and image analysis.208... 

The introduction of EU directives on Waste Electrical and Electronic Equipment and Reduction of Hazardous Substances has highlighted the need for precise and repeatable elemental analysis of heavy metals in the plastics production process. X-ray fluorescence (XRF) spectroscopy has emerged as the most economical and effective analytical tool for achieving this. A set of certified standards, known as TOXEL, is now available to facilitate XRF analyses in PE. Calibration with TOXEL standards is simplified by the fact that XRF is a multi-element technique. Therefore a single set of the new standards can be used to calibrate several heavy elements, covering concentrations from trace level to several hundred ppm. This case study is the analysis of heavy metals in PE using an Epsilon 5 XRF spectrometer. 

Cadmium in acidified aqueous solution may be analyzed at trace levels by various instrumental techniques such as flame and furnace atomic absorption, and ICP emission spectrophotometry. Cadmium in solid matrices is extracted into aqueous phase by digestion with nitric acid prior to analysis. A much lower detection level may be obtained by ICP-mass spectrometry. Other instrumental techniques to analyze this metal include neutron activation analysis and anodic stripping voltammetry. Cadmium also may be measured in aqueous matrices by colorimetry. Cadmium ions react with dithizone to form a pink-red color that can be extracted with chloroform. The absorbance of the solution is measured by a spectrophotometer and the concentration is determined from a standard calibration curve (APHA, AWWA and WEF. 1999. Standard Methods for the Examination of Water and Wastewater, 20th ed. Washington, DC American Public Health Association). The metal in the solid phase may be determined nondestructively by x-ray fluorescence or diffraction techniques. 

Silver metal and its contents in silver alloys and salts can be measured at trace levels by various instrumental techniques such as flame- and furnace-AA, ICP-AES, ICP/MS and x-ray fluorescence methods. It is solubilized by digestion with nitric acid prior to analysis. The AA measurement may be carried out at the wavelength 328.1 nm and ICP analysis at 328.07 nm. ICP/MS is the most sensitive technique while x-ray fluorescence is relatively less sen-... 

Strontium and all its compounds impart crimson red color in the flame test. The metal in trace concentrations can be analyzed by various instrumental methods that include flame-and fumace-AA, ICP-AES, ICP/MS, x-ray fluorescence, and neutron activation analysis. 

The certification procedure for seven trace metals (Ba, Ca, Li, Mg, Mn, Na and Sr) in the certified reference material FEBS-1 (National Research Council Canada, Institute for National Measurement Standards, Ottawa, Canada) based on fish otolith matrix by isotope dilution - ICP-MS in comparison to ICP optical emission spectrometry and X-ray fluorescence analysis, is described by Sturgeon et al4X The isotope dilution technique is also employed for species analysis in biological systems,46 e.g., for the determination of mercury species in tuna material,54 or in aquatic systems using cold vapour ICP-MS.55... 

The evaluation of coal mineral matter by the ashing technique can be taken further insofar as attempts can then be made to determine the individual metal constituents of the ash. On the occasion when the mineral matter has been separated from the coal successfully, it is then possible to apply any one of several techniques (such as x-ray diffraction, x-ray fluorescence, scanning electron microscopy and electron probe microanalysis) not only to investigate the major metallic elements in coal but also to investigate directly the nature (and amount) of the trace elements in the coal (Jenkins and Walker, 1978 Prather et al., 1979 Raymond and Gooley, 1979 Russell and Rimmer, 1979 Jones et al., 1992). Generally, no single method yields a complete analysis of the mineral matter in coal and it is often necessary to employ a combination of methods. 

In heavy metal analysis of all types of Day-Glo fluorescent pigments for plastics, metals were found to be present in only trace amounts (Table 16.7). The values are given in ppm of total metal present, and may vary between colors within a series. 

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